CN103855320B - A kind of organic electroluminescence device and preparation method thereof - Google Patents
A kind of organic electroluminescence device and preparation method thereof Download PDFInfo
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- CN103855320B CN103855320B CN201210501358.3A CN201210501358A CN103855320B CN 103855320 B CN103855320 B CN 103855320B CN 201210501358 A CN201210501358 A CN 201210501358A CN 103855320 B CN103855320 B CN 103855320B
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/841—Self-supporting sealing arrangements
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/846—Passivation; Containers; Encapsulations comprising getter material or desiccants
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/87—Arrangements for heating or cooling
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
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Abstract
The invention provides a kind of organic electroluminescence device; including the substrate stacked gradually, anode, functional layer, negative electrode, encapsulated layer and cap; substrate and cap are formed closes space; anode, functional layer, negative electrode and encapsulated layer are contained in this closing space, and described encapsulated layer includes protective layer, carboritride film, fluoride films, inorganic barrier layer, moist absorbing layer and heat dissipating layer successively；Described carboritride film is the nitride film doped with carbide; the material of described fluoride films is aluminium fluoride, tetrafluoride hafnium, zirconium tetrafluoride, cerium fluoride or fluorination iridium; present invention also offers the preparation method of this organic electroluminescence device; the method can efficiently reduce steam, the oxygen erosion to organic electroluminescence device; thus device organic functional material and electrode are formed and is effectively protected, the life-span of organic electroluminescence device can be significantly increased.The inventive method is particularly suited for encapsulating flexible organic electroluminescent device.
Description
Technical field
The present invention relates to electronic device association area, particularly relate to a kind of organic electroluminescence device and preparation thereof
Method.
Background technology
Organic electroluminescence device (OLED) is a kind of current mode light emitting semiconductor device based on organic material.
Its typical structure is that the luminous organic material preparing tens nanometer thickness on ito glass makees luminescent layer, on luminescent layer
There is the metal electrode of low work function side.When on electrode added with voltage, luminescent layer just produces light radiation.
It is high, low in energy consumption, light, thin, excellent without visual angle restriction etc. that OLED has active illuminating, luminous efficiency
Point, is considered to be most likely in the illumination in future and display device market by insider and occupies dominance
Device of new generation.As a brand-new illumination and Display Technique, OLED technology is in the ten years in past
Development is swift and violent, achieves huge achievement.More and more illuminate due to the whole world and show that producer puts into one after another
Research and development, have greatly promoted the industrialization process of OLED so that the growth rate of OLED industry is surprising, mesh
Before had arrived at eve of scale of mass production.
Conventional art use glass cover or crown cap are packaged, its edge ultraviolet polymerization resin seal,
But the glass cover used in this method or crown cap volume are the biggest, add the weight of device, and
The method may not apply to flexible organic electroluminescence and gives out light the encapsulation of device.
Summary of the invention
For overcoming the defect of above-mentioned prior art, the invention provides a kind of organic electroluminescence device and system thereof
Preparation Method.This organic electroluminescence device can efficiently reduce steam, organic electroluminescence is sent out by oxygen isoreactivity material
The erosion of optical device, organic functional material and the electrode of protection organic electroluminescence device exempt from destruction, to device
The life-span of part increases significantly.The inventive method is applicable to the Organic Electricity that encapsulation is prepared with conducting glass substrate
Electroluminescence device.The inventive method is particularly suited for encapsulating flexible organic electroluminescent device.
On the one hand, the invention provides a kind of organic electroluminescence device,
Including the substrate stacked gradually, anode, functional layer, negative electrode, encapsulated layer and cap, substrate and envelope
Capping is formed closes space, and anode, functional layer, negative electrode, encapsulated layer are contained in this closing space, described
Encapsulated layer includes protective layer, carboritride film, fluoride films, inorganic barrier layer, moist absorbing layer successively
And heat dissipating layer；
Described carboritride film is the nitride film doped with carbide, and wherein, described carbide material is
Carborundum, tungsten carbide, ramet, boron carbide, titanium carbide or hafnium carbide, described nitride material is four nitrogen
Change three silicon, aluminium nitride, boron nitride, silicon nitride, tantalum nitride or titanium nitride, described carbide and described nitridation
The mass ratio of thing is 1:6～14:19；The material of described fluoride films be aluminium fluoride, tetrafluoride hafnium, zirconium tetrafluoride,
Cerium fluoride or fluorination iridium.
Preferably, the thickness of described carboritride film is 80nm～150nm；The thickness of described fluoride films
For 80nm～150nm.
Preferably, the material of described protective layer is CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-
Benzidine, 8-hydroxyquinoline aluminum, silicon oxide, Afluon (Asta) or zinc sulfide, the thickness of protective layer be 200nm～
300nm；
The material of described inorganic barrier layer is politef, methacrylic resin or cycloaliphatic epoxy resin,
The thickness of described inorganic barrier layer is 1 μm～1.5 μm.
Preferably, the material of described moist absorbing layer is calcium oxide, Barium monoxide, strontium oxide or magnesium oxide, institute
The thickness stating moist absorbing layer is 100nm～200nm；
The material of described heat dissipating layer is aluminum, silver, copper or their compositions, and thickness is 200nm～500nm；
And
Described cap is foil, and the material of foil is silver, aluminum or copper.
Preferably, described carboritride film and the alternately laminated setting of described fluoride films, the stacking number of plies is more than
Equal to three layers.
Another aspect of the present invention provides the preparation method of a kind of organic electroluminescence device, comprises the following steps:
Clean glass substrate or organic film substrate are prepared the anode of organic electroluminescence device；Use
The method of vacuum evaporation is sequentially prepared functional layer, negative electrode and encapsulated layer on anode conducting substrate, uses ultraviolet
Cap is packaged by photocuring mode, makes described substrate and described cap be formed and closes space；
The preparation of described encapsulated layer includes first using the mode of vacuum evaporation to prepare protective layer on negative electrode；
Described protective layer uses magnetron sputtering spatter altogether and prepare carboritride film, described carboritride film
For the nitride film doped with carbide material, wherein, described carbide material be carborundum, tungsten carbide,
Ramet, boron carbide, titanium carbide or hafnium carbide, the nitride material in described nitride film is four nitridations three
Silicon, aluminium nitride, boron nitride, silicon nitride, tantalum nitride or titanium nitride, described magnetron sputtering condition is: use
Three target magnetic control sputtering depositing systems, arranging background vacuum is 1 × 10-5Pa～1 × 10-3Pa, thicknesses of layers sets
It is set to 80nm～150nm, is that 1:6～14:19 is as target using the mass ratio of described carbide Yu described nitride
Material, carries out magnetron sputtering under the conditions of sputter rate is 5nm/min～40nm/min and obtains carboritride film,
By the way of vacuum evaporation, fluoride films is prepared again on described carboritride film, described fluoride films
Material is aluminium fluoride, tetrafluoride hafnium, zirconium tetrafluoride, cerium fluoride or fluorination iridium, the mode of described vacuum evaporation
For vacuum 8 × 10-5Pa～3 × 10-5Pa, evaporation rate
Then the technique of first spin coating post-exposure is used to prepare inorganic barrier layer on described carboritride film, institute
The technical process stating first spin coating post-exposure is, by described Organic barrier layer material spin coating, to be then with wavelength
200nm～400nm ultraviolet light polymerization, light intensity is 10mW/cm2～15mW/cm2, time of exposure 200s～
300s；
Then sputtering mode is used to prepare moist absorbing layer, in described moisture absorption on described inorganic barrier layer
Vacuum evaporation heat dissipating layer on layer；
Finally use packaging plastic that foil encapsulation is formed cap, make described substrate and described encapsulation cap-shaped
Become confined space, described anode, functional layer, negative electrode and encapsulated layer are contained in this closing space.
Preferably, the thickness of described carboritride film is 80nm～150nm；The thickness of described fluoride films
For 80nm～150nm.
Preferably, the material of described protective layer is CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-
Benzidine, 8-hydroxyquinoline aluminum, silicon oxide, Afluon (Asta) or zinc sulfide, the thickness of protective layer be 200nm～
300nm；
The material of described inorganic barrier layer is politef, methacrylic resin or cycloaliphatic epoxy resin,
The thickness of described inorganic barrier layer is 1 μm～1.5 μm.
Preferably, the material of described moist absorbing layer is calcium oxide, Barium monoxide, strontium oxide or magnesium oxide, institute
The thickness stating moist absorbing layer is 100nm～200nm.
Preferably, the material of described heat dissipating layer is aluminum, silver, copper or their compositions, described heat dissipating layer
Thickness is 200nm～500nm.
Preferably, described cap is foil, and the material of foil is silver, aluminum or copper.
Preferably, repeat to prepare described carboritride film and the preparation technology of described fluoride films, make described
Carboritride film and described fluoride films stacking are arranged, and the alternately laminated number of plies is more than or equal to 3 layers.
The invention provides a kind of organic electroluminescence device and preparation method thereof to have the advantages that
Organic electroluminescence device of the present invention can efficiently reduce external water, oxygen isoreactivity material to Organic Electricity
The erosion of electroluminescence device, thus device organic functional material and electrode are formed and is effectively protected, significantly
Improve the life-span of organic electroluminescence device；Water resistance (WVTR) is made to reach 9.3E-5g/m2Day, the longevity
Life reaches 15, more than 713 hours, and organic electroluminescence device material of the present invention is cheap, and method for packing is simple, Yi great
Prepared by area, be suitable to industrialization large-scale use.
Accompanying drawing explanation
Fig. 1 is the structural representation of organic electroluminescence device of the present invention；
Fig. 2 is the preparation flow figure of organic electroluminescence device of the present invention；
Fig. 3 is the preparation flow figure of the encapsulated layer of organic electroluminescence device of the present invention.
Detailed description of the invention
The following stated is the preferred embodiment of the present invention.It should be pointed out that, the common skill for the art
For art personnel, under the premise without departing from the principles of the invention, it is also possible to make some improvement and adjustment, this
A little improvement and adjustment are also considered as within the scope of the present invention.
The invention provides a kind of organic electroluminescence device 100 according to Fig. 1, including the substrate 10 stacked gradually,
Anode 20, functional layer 30, negative electrode 40, encapsulated layer 50 and cap 60, substrate 10 and cap 60 form envelope
Close space, anode 20, functional layer 30, negative electrode 40 and encapsulated layer 50 are encapsulated in this space.
In the present embodiment, substrate 10 is glass substrate or organic film, and this organic film is particularly as follows: poly-right
Polyethylene terephthalate；
In the present embodiment, arranging anode 20 on the substrate 10, anode 20 is indium tin oxide；
In the present embodiment, functional layer 30 is formed at anode 20 surface.Functional layer 30 includes the sky stacked gradually
Cave implanted layer, hole transmission layer, luminescent layer, electron transfer layer, electron injecting layer.It is appreciated that hole
Implanted layer, hole transmission layer, electron transfer layer, electron injecting layer can omit, and now functional layer 30 is only wrapped
Include luminescent layer；
Hole injection layer is N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamidogen (NPB) and mixes
Miscellaneous molybdenum oxide (MoO in NPB3)。MoO3Weight/mass percentage composition be 30%.The thickness of hole injection layer
Degree is 10nm；
Hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).The thickness of hole transmission layer
For 30nm.
Emitting layer material includes material of main part and the guest materials being entrained in material of main part.Material of main part is
1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes
Iridium (Ir (ppy)3).The weight/mass percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer
For 10nm.
The material of electron injecting layer includes Bphen and the nitrine caesium (CsN being entrained in Bphen3)。CsN3's
Weight/mass percentage composition is 30%.The thickness of electron injecting layer is 20nm.
It should be noted that hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electronics note
Enter layer and can also use other materials as required.
In the present embodiment, arranging negative electrode 40 in functional layer 30, negative electrode 40 can be single metal layer, should
Single-layer metal is aluminum, silver-colored and golden；Can also be laminating transparent negative electrode, this transparent cathode be ITO/Ag/ITO or
ZnS/Ag/ZnS。
In the present embodiment, arranging encapsulated layer 50 on negative electrode 40, this encapsulated layer 50 includes protective layer 501, carbon
Nitrogen compound film 502, fluoride films 503, inorganic barrier layer 504, moist absorbing layer 505 and heat dissipating layer 506.
Protective layer 501, the material of protective layer 501 is CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl
-4,4 '-benzidine, 8-hydroxyquinoline aluminum, silicon oxide, Afluon (Asta) or zinc sulfide, the thickness of protective layer is 200
Nm～300nm.
In the present embodiment, arranging carboritride film 502 on protective layer 501, carboritride film 502 is
Doped with the carbide membrane of nitride, wherein, described carbide material be carborundum, tungsten carbide, ramet,
Boron carbide, titanium carbide or hafnium carbide, described nitride material be silicon nitride, aluminium nitride, boron nitride,
Silicon nitride, tantalum nitride or titanium nitride, described carbide is 1:6～14:19 with the mass ratio of described nitride；
In the present embodiment, the thickness of carboritride film 502 is 80nm～150nm.
In the present embodiment, at carboritride film 502 surface configuration fluorinated film, the material of described fluoride films
For aluminium fluoride, tetrafluoride hafnium, zirconium tetrafluoride, cerium fluoride or fluorination iridium.
In the present embodiment, the thickness of described fluoride films is 80nm～150nm.
In the present embodiment, described carboritride film 502 and the alternately laminated setting of fluoride films 503, alternately
The stacking number of plies is more than or equal to 3 layers.
Alternately laminated to carboritride film and fluoride films setting can be extended water Oxygen permeation path, alternately set
Put and can make up hole, make Organic substance and inorganic matter combine thus stress can be alleviated.
Fluoride films arranges inorganic barrier layer 504, the material of inorganic barrier layer 504 be politef,
Methacrylic resin or cycloaliphatic epoxy resin, thickness is 1 μm～1.5 μm.
In the present embodiment, at inorganic barrier layer 504 surface configuration moist absorbing layer 505, moist absorbing layer 505
Material be calcium oxide, Barium monoxide, strontium oxide or magnesium oxide, thickness is 100nm～200nm.
In the present embodiment, at moist absorbing layer 505 surface configuration heat dissipating layer 506, the material of heat dissipating layer 506 is
Aluminum, silver, copper or their compositions, thickness is 200nm～500nm.
In the present embodiment, use cap 60 to be packaged with substrate 10 for boundary, make substrate 10 and cap
Forming confined space between 60, above layers be arranged in this confined space, described cap 60 is metal
Thin slice, foil includes silver, aluminum or copper foil.
The preparation method of the organic electroluminescence device 100 that the present invention provides, concrete steps bag is understood according to Fig. 2
Include:
S101 prepares anode 20 on the substrate 10, and forms functional layer 30 on anode 20.
Hole injection layer that functional layer 30 includes stacking gradually, hole transmission layer, luminescent layer, electron transfer layer,
Electron injecting layer.
Substrate 10 can be substrate of glass or organic polyethylene terephthalate (PET) film substrate.
Substrate 10 has preparation has anode 20, anode 20 to be ITO layer.The thickness of ITO layer is 100nm～150nm.
Substrate 10 surface first carried out pretreatment to remove substrate 10 surface before forming anode 20 and functional layer 30
Pollutant, and carry out surface active increase substrate 10 surface oxygen content with improve substrate 10 surface work content
Number.Each ultrasonic waves for cleaning 5min of acetone, ethanol, ionized water and ethanol is gone specifically, substrate 10 used successively,
Drying up with nitrogen afterwards, baking box is dried.
In present embodiment, the material of hole injection layer includes N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-
Biphenyl-4-4 '-diamidogen (NPB) and the molybdenum oxide (MoO being entrained in NPB3)。MoO3Percent mass contain
Amount is 30%.The thickness of hole injection layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum is
3×10-5Pa, evaporation rate is
The material of hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).Hole transmission layer
Thickness be 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of luminescent layer includes material of main part and the guest materials being entrained in material of main part.Material of main part is
1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes
Iridium (Ir (ppy)3).The weight/mass percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer by
Vacuum evaporation is formed, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer
For 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
The material of electron injecting layer includes Bphen and the nitrine caesium (CsN being entrained in Bphen3), CsN3's
Weight/mass percentage composition is 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation,
Vacuum is 3 × 10-5Pa, evaporation rate is
It should be noted that hole injection layer, hole transmission layer, luminescent layer, electron transfer layer, electronics note
Enter layer and can also use other materials as required.Hole injection layer, hole transmission layer, electron transfer layer,
Electron injecting layer can omit, and now functional layer 20 only includes luminescent layer.
Step S120, functional layer 30 surface formed negative electrode 40.
Negative electrode 30 can be single layer structure.The thickness of negative electrode 30 is 100nm.The material of negative electrode 30 be aluminum (Al),
Silver (Ag) or gold (Au), negative electrode 30 is formed by vacuum evaporation, and vacuum is 5 × 10-5Pa, evaporation rate isCan also be laminating transparent negative electrode, this transparent cathode be ITO/Ag/ITO or ZnS/Ag/ZnS.
Step S130, on negative electrode 40 evaporation formed encapsulated layer 50.
According to Fig. 3, the preparation process of encapsulated layer is as follows:
Encapsulated layer includes protective layer 501, carboritride film 502, inorganic barrier layer 504, moisture absorption successively
Layer 505 and heat dissipating layer 506.
Step S1301, on negative electrode 40 evaporation formed protective layer 501, the material of protective layer 501 be CuPc,
N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine, 8-hydroxyquinoline aluminum, silicon oxide, fluorination
Magnesium or zinc sulfide, the thickness of protective layer is 200nm～300nm.Evaporation condition is, vacuum is 8 × 10-5Pa～
3×10-5Pa, evaporation rate is
Step S1302, on protective layer 502 use magnetron sputtering make carboritride film 502, carbon nitrification
Thing film 502 is the nitride film doped with carbide, wherein, described carbide material be carborundum, tungsten carbide,
Ramet, boron carbide, titanium carbide or hafnium carbide, described nitride material be silicon nitride, aluminium nitride,
Boron nitride, silicon nitride, tantalum nitride or titanium nitride, the mass ratio of described carbide and described nitride be 1:6～
14:19.Wherein, magnetron sputtering condition is: uses three target magnetic control sputtering depositing systems, arranges background vacuum
It is 1 × 10-5Pa～1 × 10-3Pa, thicknesses of layers is set to 80nm～150nm, by carbide and nitride
Mass ratio is 1:6～14:19 as target, is that 5nm/min-40nm/min carries out magnetron sputtering and obtains at sputter rate
To carboritride film 502.
Step S1303, it is evaporated in vacuo fluoride films 503, the material of described fluoride films at carboritride film 502
Material is aluminium fluoride, tetrafluoride hafnium, zirconium tetrafluoride, cerium fluoride or fluorination iridium, and the mode of described vacuum evaporation is
Vacuum 8 × 10-5Pa～3 × 10-5Pa, evaporation rate
Step S1304, at fluoride films 503 spin coating inorganic barrier layer 504, use purple the most under an inert atmosphere
Outer photocuring, ultraviolet light polymerization condition is wavelength 200nm～400nm, light intensity 10mW/cm2～15
mW/cm2, time of exposure 200s～300s, inorganic barrier layer 504 thickness is 1 μm～1.5 μm；
Step S1305, using sputtering mode to prepare moist absorbing layer 505 on inorganic barrier layer 504, dampness is inhaled
The material receiving layer 505 is calcium oxide, Barium monoxide, strontium oxide or magnesium oxide, and thickness is 100nm～200nm.
Sputtering condition is that described sputtering mode is specially vacuum 1 × 10-5Pa～1 × 10-3Pa, steams firing rate degree
Step S1306, on moist absorbing layer 505 use evaporation mode prepare heat dissipating layer 506, heat dissipating layer 506
Material be aluminum, silver, copper or their compositions, thickness is 200nm～500nm.Evaporation condition is, very
Reciprocal of duty cycle is 8 × 10-5Pa～3 × 10-5Pa, evaporation rate
In a preferred embodiment, by being alternately repeated step S1303 and step S1304 prepares what stacking was arranged
Carboritride film 502 and fluoride films 503, the alternately laminated number of plies is more than or equal to 3 layers；
Encapsulated layer is formed by step S1302 to step S1306；
Step S140, encapsulated layer 50 surface formed cap 60.
At cap edge coating cloth packaging plastic, the mode of ultraviolet curing is used to harden packaging plastic, purple
A length of 200nm～400nm of outer light wave, light intensity is 10mW/cm2～15mW/cm2, time of exposure 300s～
400s, makes to be formed between cap 60 and substrate 10 confined space.
Embodiment 1:
The preparation method of a kind of organic electroluminescence device, comprises the following steps:
1, substrate pre-treatment and the preparation of anode: use acetone, ethanol, deionized water and ethanol to use successively
Ultrasonic washing unit is carried out, and washing scavenging period is 5 minutes every time, then dries up with nitrogen, uses and dries
Case is stand-by after drying；Substrate arranges ito glass, the substrate being loaded with ito glass is carried out surface active
Process, to increase the oxygen content of surface layer, improve the work function of anode surface；Ito glass thickness is 100nm；
2, the preparation of functional layer:
Anode is deposited with hole injection layer；
The material of hole injection layer includes N, N '-two (1-naphthyl)-N, N '-diphenyl-1,1 '-biphenyl-4-4 '-diamidogen
And the molybdenum oxide (MoO that is entrained in NPB (NPB)3)。MoO3Weight/mass percentage composition be 30%.Empty
The thickness of cave implanted layer is 10nm.Hole injection layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation
Speed is
Hole injection layer is deposited with hole transmission layer；
The material of hole transmission layer is 4,4', 4 " and-three (carbazole-9-base) triphenylamine (TCTA).Hole transmission layer
Thickness be 30nm.Hole transmission layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, and evaporation rate is
Hole transmission layer is deposited with luminescent layer；
The material of luminescent layer includes material of main part and the guest materials being entrained in material of main part.Material of main part is
1,3,5-tri-(1-phenyl-1H-benzimidazolyl-2 radicals-yl) benzene (TPBI), guest materials is that three (2-phenylpyridine) closes
Iridium (Ir (ppy)3).The weight/mass percentage composition of guest materials is 5%.The thickness of luminescent layer is 20nm.Luminescent layer by
Vacuum evaporation is formed, and vacuum is 3 × 10-5Pa, evaporation rate is
Luminescent layer is deposited with electron transfer layer；
The material of electron transfer layer is 4,7-diphenyl-1,10-phenanthroline (Bphen).The thickness of electron transfer layer
For 10nm.Electron transfer layer is formed by vacuum evaporation, and vacuum is 3 × 10-5Pa, evaporation rate is
It is deposited with electron injecting layer on the electron transport layer；
The material of electron injecting layer includes Bphen and the nitrine caesium (CsN3) being entrained in Bphen, CsN3's
Weight/mass percentage composition is 30%.The thickness of electron injecting layer is 20nm.Electron injecting layer is formed by vacuum evaporation,
Vacuum is 3 × 10-5Pa, evaporation rate is
3, evaporation cathode on electron injecting layer:
Metallic cathode uses aluminum (Al), and thickness is 100nm, and evaporation vacuum is 5 × 10-5Pa, evaporation rate is
4, the preparation of encapsulated layer:
Arranging encapsulated layer on negative electrode, encapsulated layer includes protective layer, carboritride film, fluoride films, has
Machine barrier layer, moist absorbing layer and heat dissipating layer；
On negative electrode, evaporation forms protective layer, and the material of protective layer is CuPc, and the thickness of protective layer is 200nm.
Evaporation condition is, vacuum is 3 × 10-5Pa, evaporation rate is
Using magnetron sputtering to make carboritride film on the protection layer, carboritride film is doped with carbonization
The nitride film of thing, wherein, carbide material is carborundum, and nitride material is silicon nitride, carbonization
Thing is 1:4 with the mass ratio of described nitride.Wherein, magnetron sputtering condition is: use three target magnetic control sputterings to sink
Long-pending system, arranging background vacuum is 1 × 10-5Pa, thicknesses of layers is set to 120nm, at sputter rate is
5nm/min carries out magnetron sputtering and obtains carboritride film.
Being evaporated in vacuo fluoride films on carboritride film, the material of fluoride films is aluminium fluoride, and vacuum is steamed
The vacuum sent out is 5 × 10-5Pa, evaporation rateThickness 100nm；
Spin coating inorganic barrier layer on fluoride films, Organic barrier layer material is politef, then lazy
Property atmosphere under use ultraviolet light polymerization, ultraviolet light polymerization condition is wavelength 365nm, light intensity 10mW/cm2, expose
Light time 200s, Organic barrier layer thickness is 1 μm；
Alternately preparation three times of carboritride film and fluoride films；
Using sputtering mode to prepare moist absorbing layer on inorganic barrier layer, the material of moist absorbing layer is oxidation
Calcium, thickness is 200nm.Sputtering condition is that described sputtering mode is specially vacuum 2 × 10-4Pa, steams firing rate degree
Using evaporation mode to prepare heat dissipating layer on moist absorbing layer, the material of heat dissipating layer is aluminum, and thickness is 200
nm.Evaporation condition is, vacuum is 5 × 10-5Pa, evaporation rate
5, the preparation of cap:
At cap edge coating cloth packaging plastic, the mode of ultraviolet curing is used to harden packaging plastic, purple
The a length of 365nm of outer light wave, light intensity is 11mW/cm2, time of exposure 350s, make shape between cap and substrate
Become confined space.
Embodiment 2:
The preparation method of a kind of organic electroluminescence device, comprises the following steps:
1,2,3 with embodiment 1；
4, the preparation of encapsulated layer:
Negative electrode arranges encapsulated layer, encapsulated layer include protective layer, carboritride film, inorganic barrier layer,
Moist absorbing layer and heat dissipating layer；
On negative electrode, evaporation forms protective layer, and the material of protective layer is N, N '-(1-naphthyl)-N, N '-hexichol
Base-4,4 '-benzidine, the thickness of protective layer is 300nm.Evaporation condition is, vacuum is 3 × 10-5Pa, steams
Sending out speed is
Using magnetron sputtering to make carboritride film on the protection layer, carboritride film is doped with carbonization
The nitride film of thing, wherein, carbide material is tungsten carbide, and nitride material is aluminium nitride, carbide with
The mass ratio of described nitride is 1:19.Wherein, magnetron sputtering condition is: use three target magnetic control sputterings to deposit system
System, arranging background vacuum is 2 × 10-4Pa, thicknesses of layers is set to 100nm, is 1nm/min at sputter rate
Carry out magnetron sputtering and obtain carboritride film.
Being evaporated in vacuo fluoride films on carboritride film, the material of fluoride films is tetrafluoride hafnium, vacuum
The vacuum of evaporation is 5 × 10-5Pa, evaporation rateThickness 80nm；
Spin coating inorganic barrier layer on fluoride films, Organic barrier layer material is methacrylic resin, then
Using ultraviolet light polymerization, ultraviolet light polymerization condition under an inert atmosphere is wavelength 365nm, light intensity 15mW/cm2,
Time of exposure 200s, Organic barrier layer thickness is 1.5 μm；
Alternately preparation three times of carboritride film and fluoride films；
Using sputtering mode to prepare moist absorbing layer on inorganic barrier layer, the material of moist absorbing layer is oxidation
Barium, thickness is 200nm.Sputtering condition is that described sputtering mode is specially vacuum 2 × 10-4Pa, steams firing rate degree
Using evaporation mode to prepare heat dissipating layer on moist absorbing layer, the material of heat dissipating layer is silver, and thickness is 500
nm.Evaporation condition is, vacuum is 5 × 10-5Pa, evaporation rate
5, the preparation of cap:
At cap edge coating cloth packaging plastic, the material of cap is aluminum slice, uses ultraviolet light polymerization to do
Dry mode is hardened packaging plastic, and a length of 365nm of ultraviolet light wave, light intensity is 10mW/cm2, time of exposure 400s,
Make to be formed between cap and substrate confined space.
Embodiment 3:
The preparation method of a kind of organic electroluminescence device, comprises the following steps:
1,2,3 with embodiment 1；
4, the preparation of encapsulated layer:
Negative electrode arranges encapsulated layer, encapsulated layer include protective layer, carboritride film, inorganic barrier layer,
Moist absorbing layer and heat dissipating layer；
On negative electrode, evaporation forms protective layer, and the material of protective layer is 8-hydroxyquinoline aluminum, the thickness of protective layer
For 250nm.Evaporation condition is, vacuum is 3 × 10-5Pa, evaporation rate is
Using magnetron sputtering to make carboritride film on the protection layer, carboritride film is doped with carbonization
The nitride film of thing, wherein, carbide material is ramet, and nitride material is boron nitride, carbide with
The mass ratio of described nitride is 3:7.Wherein, magnetron sputtering condition is: use three target magnetic control sputterings to deposit system
System, arranging background vacuum is 2 × 10-4Pa, thicknesses of layers is set to 150nm, at sputter rate is
40nm/min carries out magnetron sputtering and obtains carboritride film.
Being evaporated in vacuo fluoride films on carboritride film, the material of fluoride films is cerium fluoride, and vacuum is steamed
The vacuum sent out is 5 × 10-5Pa, evaporation rateThickness 150nm；
Spin coating inorganic barrier layer on fluoride films, Organic barrier layer material is cycloaliphatic epoxy resin, then
Using ultraviolet light polymerization, ultraviolet light polymerization condition under an inert atmosphere is wavelength 365nm, light intensity 11mW/cm2,
Time of exposure 230s, Organic barrier layer thickness is 1.2 μm；
Alternately preparation four times of carboritride film and fluoride films；
Using sputtering mode to prepare moist absorbing layer on inorganic barrier layer, the material of moist absorbing layer is oxidation
Strontium, thickness is 150nm.Sputtering condition is that described sputtering mode is specially vacuum 2 × 10-4Pa, steams firing rate degree
Using evaporation mode to prepare heat dissipating layer on moist absorbing layer, the material of heat dissipating layer is copper, and thickness is 300
nm.Evaporation condition is, vacuum is 5 × 10-5Pa, evaporation rate
5, the preparation of cap:
At cap edge coating cloth packaging plastic, the material of cap is copper foil, uses ultraviolet light polymerization to do
Dry mode is hardened packaging plastic, and a length of 365nm of ultraviolet light wave, light intensity is 15mW/cm2, time of exposure 300s,
Make to be formed between cap and substrate confined space.
Embodiment 4:
The preparation method of a kind of organic electroluminescence device, comprises the following steps:
1,2,3 with embodiment 1；
4, the preparation of encapsulated layer:
Negative electrode arranges encapsulated layer, encapsulated layer include protective layer, carboritride film, inorganic barrier layer,
Moist absorbing layer and heat dissipating layer；
On negative electrode, evaporation forms protective layer, and the material of protective layer is silicon oxide, and the thickness of protective layer is 200nm.
Evaporation condition is, vacuum is 5 × 10-5Pa, evaporation rate is
Using magnetron sputtering to make carboritride film on the protection layer, carboritride film is doped with carbonization
The nitride film of thing, wherein, carbide material is boron carbide, and nitride material is silicon nitride, carbide with
The mass ratio of described nitride is 1:4.Wherein, magnetron sputtering condition is: use three target magnetic control sputterings to deposit system
System, arranging background vacuum is 2 × 10-4Pa, thicknesses of layers is set to 120nm, at sputter rate is
20nm/min carries out magnetron sputtering and obtains carboritride film.
Being evaporated in vacuo fluoride films on carboritride film, the material of fluoride films is cerium fluoride, and vacuum is steamed
The vacuum sent out is 5 × 10-5Pa, evaporation rateThickness 120nm；
Spin coating inorganic barrier layer on fluoride films, Organic barrier layer material is politef, then lazy
Property atmosphere under use ultraviolet light polymerization, ultraviolet light polymerization condition is wavelength 365nm, light intensity 10mW/cm2, expose
Light time 200s, Organic barrier layer thickness is 1 μm；
Alternately preparation five times of carboritride film and fluoride films；
Using sputtering mode to prepare moist absorbing layer on inorganic barrier layer, the material of moist absorbing layer is oxidation
Magnesium, thickness is 100nm.Sputtering condition is that described sputtering mode is specially vacuum 2 × 10-4Pa, steams firing rate degree
Using evaporation mode to prepare heat dissipating layer on moist absorbing layer, the material of heat dissipating layer is albronze, copper
Being 3:1 with the mass ratio of aluminum, thickness is 500nm.Evaporation condition is, vacuum is 5 × 10-5Pa, evaporation rate
5, the preparation of cap:
At cap edge coating cloth packaging plastic, the material of cap is copper foil, uses ultraviolet light polymerization to do
Dry mode is hardened packaging plastic, and a length of 365nm of ultraviolet light wave, light intensity is 11mW/cm2, time of exposure 350s,
Make to be formed between cap and substrate confined space.
Embodiment 5:
The preparation method of a kind of organic electroluminescence device, comprises the following steps:
1,2,3 with embodiment 1；
4, the preparation of encapsulated layer:
Negative electrode arranges encapsulated layer, encapsulated layer include protective layer, carboritride film, inorganic barrier layer,
Moist absorbing layer and heat dissipating layer；
On negative electrode, evaporation forms protective layer, and the material of protective layer is Afluon (Asta), and the thickness of protective layer is 300nm.
Evaporation condition is, vacuum is 5 × 10-5Pa, evaporation rate is
Using magnetron sputtering to make carboritride film on the protection layer, carboritride film is doped with carbonization
The nitride film of thing, wherein, carbide material is titanium carbide, and nitride material is tantalum nitride, carbide with
The mass ratio of described nitride is 1:9.Wherein, magnetron sputtering condition is: use three target magnetic control sputterings to deposit system
System, arranging background vacuum is 2 × 10-4Pa, thicknesses of layers is set to 110nm, is 1nm/min at sputter rate
Carry out magnetron sputtering and obtain carboritride film.
Being evaporated in vacuo fluoride films on carboritride film, the material of fluoride films steams for fluorination iridium, vacuum
The vacuum sent out is 5 × 10-5Pa, evaporation rateThickness 100nm；
Spin coating inorganic barrier layer on fluoride films, Organic barrier layer material is methacrylic resin, then
Using ultraviolet light polymerization, ultraviolet light polymerization condition under an inert atmosphere is wavelength 365nm, light intensity 15mW/cm2,
Time of exposure 200s, Organic barrier layer thickness is 1.5 μm；
Using sputtering mode to prepare moist absorbing layer on inorganic barrier layer, the material of moist absorbing layer is oxidation
Calcium, thickness is 200nm.Sputtering condition is that described sputtering mode is specially vacuum 2 × 10-4Pa, steams firing rate degree
Using evaporation mode to prepare heat dissipating layer on moist absorbing layer, the material of heat dissipating layer is albronze, copper
Being 3:1 with the mass ratio of aluminum, thickness is 500nm.Evaporation condition is, vacuum is 5 × 10-5Pa, evaporation rate
5, the preparation of cap:
At cap edge coating cloth packaging plastic, the material of cap is copper foil, uses ultraviolet light polymerization to do
Dry mode is hardened packaging plastic, and a length of 365nm of ultraviolet light wave, light intensity is 15mW/cm2, time of exposure 400s,
Make to be formed between cap and substrate confined space.
Embodiment 6:
The preparation method of a kind of organic electroluminescence device, comprises the following steps:
1,2,3 with embodiment 1；
4, the preparation of encapsulated layer:
Negative electrode arranges encapsulated layer, encapsulated layer include protective layer, carboritride film, inorganic barrier layer,
Moist absorbing layer and heat dissipating layer；
On negative electrode, evaporation forms protective layer, and the material of protective layer is zinc sulfide, and the thickness of protective layer is 250nm.
Evaporation condition is, vacuum is 5 × 10-5Pa, evaporation rate is
Using magnetron sputtering to make carboritride film on the protection layer, carboritride film is doped with carbonization
The nitride film of thing, wherein, carbide material is hafnium carbide, and nitride material is titanium nitride, carbide with
The mass ratio of described nitride is 3:17.Wherein, magnetron sputtering condition is: use three target magnetic control sputterings to deposit system
System, arranging background vacuum is 2 × 10-4Pa, thicknesses of layers is set to 130nm, is 5nm/min at sputter rate
Carry out magnetron sputtering and obtain carboritride film.
Being evaporated in vacuo fluoride films on carboritride film, the material of fluoride films is cerium fluoride, and vacuum is steamed
The vacuum sent out is 5 × 10-5Pa, evaporation rateThickness 100nm；
Spin coating inorganic barrier layer on fluoride films, Organic barrier layer material is cycloaliphatic epoxy resin, then
Using ultraviolet light polymerization, ultraviolet light polymerization condition under an inert atmosphere is wavelength 365nm, light intensity 11mW/cm2,
Time of exposure 230s, Organic barrier layer thickness is 1.2 μm；
Using sputtering mode to prepare moist absorbing layer on inorganic barrier layer, the material of moist absorbing layer is oxidation
Barium, thickness is 150nm.Sputtering condition is that described sputtering mode is specially vacuum 2 × 10-4Pa, steams firing rate degree
Using evaporation mode to prepare heat dissipating layer on moist absorbing layer, the material of heat dissipating layer is silver, and thickness is 300
nm.Evaporation condition is, vacuum is 5 × 10-5Pa, evaporation rate
Alternately preparation eight times of carboritride film and fluoride films；
5, the preparation of cap:
At cap edge coating cloth packaging plastic, the material of cap is copper foil, uses ultraviolet light polymerization to do
Dry mode is hardened packaging plastic, and a length of 365nm of ultraviolet light wave, light intensity is 11mW/cm2, time of exposure 350s,
Make to be formed between cap and substrate confined space.
Effect example
Beneficial effect for valid certificates organic electroluminescence device of the present invention and preparation method thereof, it is provided that relevant
Experimental data is as follows.
The test condition of organic electroluminescence device water oxygen permeability is: equipment: Keithley company
Keithley2400, specimen holder；Method: the change of test Ca membrane resistance；Condition: temperature 20 DEG C～25 DEG C,
Humidity 40%～60%.Result is as follows:
Table 1. embodiment 1～6 organic electroluminescence device water oxygen permeability
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| WVTR(g/m2/day) | 8.4E-5 | 7.1E-5 | 9.3E-5 | 8.0E-5 | 5.1E-5 | 7.7E-5 |
Table 1 is embodiment 1～6 organic electroluminescence device water oxygen permeability, makes water resistance (WVTR)
Reach 9.3E-5g/m2·day。
Organic electro-luminescence device lifetime test condition: equipment: the Keithley2400 of Keithley company, Ke Ni
The CS-100A colorimeter of card Minolta company；Method: test brightness is from 1000cd/m2Drop to 700cd/m2
Time used；Condition: temperature 20 DEG C～25 DEG C, humidity 40%～60%.
Table 2. embodiment 1～6 organic electro-luminescence device lifetime situation
Table 2 is embodiment 1～6 organic electro-luminescence device lifetime situation it can be seen that organic electroluminescence of the present invention
The life-span of luminescent device reaches more than 1.5713 ten thousand hours (T70@1000cd/m2)。
To sum up, the organic electroluminescence device that the present invention provides can efficiently reduce external water, oxygen isoreactivity thing
The erosion of confrontation organic electroluminescence device, thus device organic functional material and electrode are formed effective guarantor
Protect, meet the sealing requirements of encapsulation, the life-span of OLED can be significantly increased.
Claims (10)
1. an organic electroluminescence device, including the substrate stacked gradually, anode, functional layer, negative electrode,
Encapsulated layer and cap, substrate and cap are formed closes space, anode, functional layer, negative electrode, encapsulated layer
It is contained in this closing space, it is characterised in that described encapsulated layer includes protective layer, carboritride successively
Film, fluoride films, inorganic barrier layer, moist absorbing layer and heat dissipating layer；
Described carboritride film is the nitride film doped with carbide, and wherein, described carbide material is
Carborundum, tungsten carbide, ramet, boron carbide, titanium carbide or hafnium carbide, described nitride material is four nitrogen
Change three silicon, aluminium nitride, boron nitride, silicon nitride, tantalum nitride or titanium nitride, described carbide and described nitridation
The mass ratio of thing is 1:6～14:19；The material of described fluoride films be aluminium fluoride, tetrafluoride hafnium, zirconium tetrafluoride,
Cerium fluoride or fluorination iridium.
2. organic electroluminescence device as claimed in claim 1, it is characterised in that described carboritride
The thickness of film is 80nm～150nm；The thickness of described fluoride films is 80nm～150nm.
3. organic electroluminescence device as claimed in claim 1, it is characterised in that the material of described protective layer
Material for CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine, 8-hydroxyquinoline aluminum,
Silicon oxide, Afluon (Asta) or zinc sulfide, the thickness of protective layer is 200nm～300nm；
The material of described inorganic barrier layer is politef, methacrylic resin or cycloaliphatic epoxy resin,
The thickness of described inorganic barrier layer is 1 μm～1.5 μm.
4. organic electroluminescence device as claimed in claim 1, it is characterised in that described moist absorbing layer
Material be calcium oxide, Barium monoxide, strontium oxide or magnesium oxide, described moisture absorption layer thickness be 100nm～
200nm；
The material of described heat dissipating layer is aluminum, silver, copper or their compositions, and the thickness of described heat dissipating layer is
200nm～500nm；And
Described cap is foil, and the material of foil is silver, aluminum or copper.
5. organic electroluminescence device as claimed in claim 1, it is characterised in that described carboritride
Film and the alternately laminated setting of described fluoride films, the stacking number of plies is more than or equal to three layers.
6. the preparation method of an organic electroluminescence device, it is characterised in that comprise the following steps:
Clean glass substrate or organic film substrate are prepared the anode of organic electroluminescence device；Use
The method of vacuum evaporation is sequentially prepared functional layer, negative electrode and encapsulated layer on anode conducting substrate, uses ultraviolet
Cap is packaged by photocuring mode, makes described substrate and described cap be formed and closes space；
The preparation of described encapsulated layer includes first using the mode of vacuum evaporation to prepare protective layer on negative electrode；
Described protective layer uses magnetron sputtering spatter altogether and prepare carboritride film, described carboritride film
For the nitride film doped with carbide material, wherein, described carbide material be carborundum, tungsten carbide,
Ramet, boron carbide, titanium carbide or hafnium carbide, the nitride material in described nitride film is four nitridations three
Silicon, aluminium nitride, boron nitride, silicon nitride, tantalum nitride or titanium nitride, described magnetron sputtering condition is: use
Three target magnetic control sputtering depositing systems, arranging background vacuum is 1 × 10-5Pa～1 × 10-3Pa, thicknesses of layers sets
It is set to 80nm～150nm, is that 1:6～14:19 is as target using the mass ratio of described carbide Yu described nitride
Material, carries out magnetron sputtering under the conditions of sputter rate is 5nm/min～40nm/min and obtains carboritride film,
By the way of vacuum evaporation, fluoride films is prepared again on described carboritride film, described fluoride films
Material is aluminium fluoride, tetrafluoride hafnium, zirconium tetrafluoride, cerium fluoride or fluorination iridium, the mode of described vacuum evaporation
For vacuum 8 × 10-5Pa～3 × 10-5Pa, evaporation rate
Then the technique of first spin coating post-exposure is used to prepare inorganic barrier layer, described elder generation on described fluoride films
The technical process of spin coating post-exposure is, by described Organic barrier layer material spin coating, then with wavelength be 200nm～
400nm ultraviolet light polymerization, light intensity is 10mW/cm2～15mW/cm2, time of exposure 200s～300s；
Then sputtering mode is used to prepare moist absorbing layer, in described moisture absorption on described inorganic barrier layer
Vacuum evaporation heat dissipating layer on layer；
Finally use packaging plastic that foil encapsulation is formed cap, make described substrate and described encapsulation cap-shaped
Become confined space, described anode, functional layer, negative electrode and encapsulated layer are contained in this closing space.
7. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterised in that described
The thickness of carboritride film is 80nm～150nm；The thickness of described fluoride films is 80nm～150nm.
8. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterised in that described
The material of protective layer is CuPc, N, N '-(1-naphthyl)-N, N '-diphenyl-4,4 '-benzidine, eight hydroxyls
Base quinoline aluminum, silicon oxide, Afluon (Asta) or zinc sulfide, the thickness of protective layer is 200nm～300nm；
The material of described inorganic barrier layer is politef, methacrylic resin or cycloaliphatic epoxy resin,
The thickness of described inorganic barrier layer is 1 μm～1.5 μm.
9. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterised in that described
The material of moist absorbing layer is calcium oxide, Barium monoxide, strontium oxide or magnesium oxide, the thickness of described moist absorbing layer
Degree is 100nm～200nm, and the material of described heat dissipating layer is aluminum, silver, copper or their compositions, described scattered
The thickness of thermosphere is 200nm～500nm, and described cap is foil, the material of foil be silver,
Aluminum or copper.
10. the preparation method of organic electroluminescence device as claimed in claim 6, it is characterised in that repeat
Prepare described carboritride film and the preparation technology of described fluoride films, make described carboritride film and institute
Stating fluoride films stacking to arrange, the alternately laminated number of plies is more than or equal to 3 layers.
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